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采用电化学法,合成出含双键聚硅烷与不含双键聚硅烷,通过FT-IR,UV,1HNMR表征其结构。分别研究了电化学反应体系和直接化学反应体系中Si-Cl键含量的变化,以及加入引发剂蒽对反应速率的影响。结果表明:含双键聚硅烷的合成反应速率快于不含双键的聚硅烷,相同反应电量下含双键聚硅烷反应体系中的Si-Cl键含量比不含双键聚硅烷少10%~15%;在电化学合成聚硅烷的过程中,单体与镁发生的格氏反应在整个反应中占有相当的比例;引发剂蒽的加入能够有效地提高不含双键聚硅烷的反应速率。本文还对电化学合成聚硅烷的反应机理进行了推测。
Electrochemical methods were used to synthesize polysiloxanes with double bonds and polysilanes without double bonds, and their structures were characterized by FT-IR, UV and 1HNMR. The changes of Si-Cl bond content in the electrochemical reaction system and the direct chemical reaction system, respectively, and the effect of the addition of the initiator anthracene on the reaction rate were studied. The results show that the synthesis rate of polysiloxane containing double bonds is faster than that of polysilane containing no double bonds. The content of Si-Cl bonds in double-bond polysilane reaction system with the same reaction charge is less than 10% ~ 15%. During the electrochemical synthesis of polysilane, the Grignard reaction between monomer and magnesium occupies a considerable proportion of the total reaction; the addition of initiator anthracene can effectively improve the reaction rate of double bond-free polysilane . The reaction mechanism of electrochemical synthesis of polysilane was also speculated.